反应详情

8.3 g (0.12 mol) of hydroxylamine hydrochloride are dissolved in 50 ml of water and treated with 10.1 g (0.12 mol) of sodium bicarbonate. This solution (pH 6-7) is added at room temperature while stirring to a solution of 14.3 g (0.1 mol) of 3-methyl-3-thiocyanato-2-butanone in 100 ml of ethanol. The temperature of the mixture rises rapidly to 37° C. The mixture is subsequently stirred for an additional 1 hour and 120 mlof the solvent are distilled off at 50° C. under reduced pressure. The residue is extracted three times with 100 ml of diethyl ether each time and the organic phase is washed with a small amount of water, dried over anhydrous sodium sulfate and concentrated until crystallization begins. After cooling, the crystal slurry is treated with 10 ml of n-hexane. The crystals are filtered off under suction, washed with diethylether/n-hexane (2:1) and dried to yield 2-oxo-4,5,5-trimethyl-3-thiazoline oxime, m.p. 151°-153° C.

1. customrises rapidly to 37° C
2. distillation120 mlof the solvent are distilled off at 50° C. under reduced pressure
3. extractionThe residue is extracted three times with 100 ml of diethyl ether each time
4. washthe organic phase is washed with a small amount of water
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated until crystallization
7. temperatureAfter cooling
8. additionthe crystal slurry is treated with 10 ml of n-hexane
9. filtrationThe crystals are filtered off under suction
10. washwashed with diethylether/n-hexane (2:1)
11. customdried